超高效液相色谱 - 串联质谱法快速检测鳗鱼中.PDFVIP

※分析检测 食品科学 2009, Vol. 30, No. 14 167 刘正才，杨 方，余孔捷，李耀平，林永辉，张 琼，刘素珍 (福建出入境检验检疫局，福建 福州 350001) 建立鳗鱼中 15 种磺胺、3 种喹诺酮类以及 4 种四环素族抗生素残留的超高效液相色谱 - 串联质谱同时测定 方法。采用酸性 EDTA-Mcllvaine 缓冲液提取，经 HLB 固相萃取小柱富积、净化后进行UPLC 分离，电喷雾串联 质谱进行检测，多离子反应监测(MRM)模式定量。添加水平为 5 、10、20 μg/kg 时各种化合物的平均回收率范围 为 72.4% ～97.3% ，RSD 值均小于 14.4% 。该法简单、快速、灵敏，适用于鳗鱼中多磺胺组分、喹诺酮及四环 素族组分残留的同时测定。 超高效液相色谱串联质谱法(UPLC-MS-MS) ；磺胺类；喹诺酮类；四环素族；鳗鱼 Simultaneous Determination of Qunolones, Sulfonamides and Tetracyclines Residues in Eel Using Solid Phase Extraction (SPE) and Ultra-performance Liquid Chromatography-Electrospray Tandem Mass Spectrometry (UPLC-MS-MS) LIU Zheng-cai ，YANG Fang ，YU Kong-jie ，LI Yao-ping ，LIN Yong-hui ，ZHANG Qiong ，LIU Su-zhen (Fujian Entry-Exit Inspection and Quarantine Bureau, Fuzhou 350001, China) Abstract ：A robust and sensitive UPLC-MS-MS method was developed for the simultaneous determination of residues of 15 sulfonamides, 3 fluoroquinolones and 4 tetracylines in eel. The target compounds were extracted with acidic EDTA-Mcllvaine buffer solution, and enriched and cleared up using a hydrophilic-lipophilic balance (HLB) SPE cartridge. After seperation on UPLC BEH C18, the analytes were detected using a tandem mass spectrometry and quantified in multiple reaction monitoring (MRM) mode. At the spike levels of 5, 10 and 20 μg/kg respectively, the average recoveries for all the compounds were 72.4% －97.3%, and the variation coefficients were all under 14.4%. This method is simple, fast, sensitive, and particular for the simulaneous determination of sulfonamides, fluoroquinolones and tetracylines in eel. Key words ：ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS-MS) ；sulfonamides ； qunolones ；tetr